A kind of graphene/sio2 hybrid polyimide foam material and preparation method thereof

A technology of polyimide and foam material, which is applied in the field of graphene/SiO2 hybrid polyimide foam material and its preparation, can solve the problems such as compound preparation of hybrid foam material which has not yet been considered, and achieves shortening of heat conduction time, foaming and so on. The effect of uniform pore structure and fast heating rate

Active Publication Date: 2019-04-30
陕西工业职业技术学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, so far people have not considered the composite of graphene, nano-silica, and polyimide to prepare hybrid foam materials.

Method used

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  • A kind of graphene/sio2 hybrid polyimide foam material and preparation method thereof
  • A kind of graphene/sio2 hybrid polyimide foam material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0047] S1. Dissolve 10g flake graphite powder and 3.5g sodium nitrate in 200mL concentrated H2SO4, put the concentrated H2SO4 into a 1000mL three-neck flask in advance, cool to 0°C in an ice bath, and ultrasonically treat for 1h;

[0048] S2. Add 40g KMnO4, react at 4°C for 1.5h, then adjust the temperature to 38°C, and ultrasonically react for 30min;

[0049] S3. Add the mixed solution obtained in S2 into 500mL of deionized water, then control the temperature at 95°C, and stir mechanically for 30min;

[0050] S4. Add 600mL deionized water to stop the reaction, then add 30mL hydrogen peroxide with a volume fraction of 30%, and continue the reaction until no gas is produced;

[0051] S5. Use the mixed acid solution of H2O:H2O2:H2SO4=l:0.23:0.26 to purify the solution obtained in S4 for 15 times, wash with low-speed centrifugation to remove excess acid and by-products, and then disperse the neutral graphite oxide in distilled water During the stripping by ultrasonic vibration f...

Embodiment 2

[0056] S1. Dissolve 10g of graphite powder and 3.5g of sodium nitrate in 200mL of concentrated H2SO4, and ultrasonically treat for 1.5h at 0°C;

[0057] S2. Add 40g KMnO4, react at 5°C for 2h, then adjust the temperature to 35°C, and react with ultrasonic oscillation for 60min;

[0058] S3. Add the mixed solution obtained in S2 into 500mL of deionized water, then control the temperature at 90°C, and stir mechanically for 60min;

[0059] S4. Add 600mL deionized water to stop the reaction, then add 30mL hydrogen peroxide with a volume fraction of 30%, and continue the reaction until no gas is produced;

[0060] S5. Purify the solution obtained in S5 15 times with a mixed acid solution of H2O:H2O2:H2SO4=1:0.23:0.26, then disperse in distilled water, ultrasonically vibrate for 60min, centrifuge, and extract the GO aqueous solution;

[0061] S6. air-drying at room temperature for 12 hours to obtain anhydrous graphene oxide sheet, and to grind it into powder;

[0062] S7. Weigh 20...

Embodiment 3

[0065] M1. Add 32.2gBTDA to 15mg methanol, heat at 70°C for 2h, then add 19.8gODA, continue heating at 70°C for 2h, then add 0.025g of 3-aminopropyltriethoxysilane dropwise, Continue to react for 1h;

[0066] M2. add the prepared modified graphene oxide of 10mg embodiment 1, continue reaction 1h, add 6.5mgTEOS, continue reaction 30min, obtain graphene / SiO The precursor solution of hybrid polyimide foam material;

[0067] M3. Heat the precursor solution described in M2, remove excess solvent, use a pulverizer to grind and sieve the dried precursor to obtain a precursor powder with uniform particle size;

[0068] M4. Put the precursor powder into a self-made mold, foam and imidize in a microwave oven to prepare a graphene / SiO2 hybrid polyimide foam material.

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Abstract

The invention discloses a graphene / SiO2 hybrid polyimide foam material and a preparation method thereof. The graphene / SiO2 hybrid polyimide foam material is prepared from modified graphene oxide, benzophenone tetracarboxylic acid dianhydride, diaminodiphenyl ether, 3-aminopropyltriethoxysilane and tetraethoxysilane through an amidation reaction and a sol-gel reaction. The modified graphene oxide is modified graphene oxide with the surface containing isocyanato. On the one hand, the prepared graphene / SiO2 hybrid polyimide foam material fully exerts the good enhancing effect of the graphene oxide and the good toughening effect of silicon dioxide, on the other hand, the defect that the graphene oxide and silicon dioxide are prone to cluster is overcome, SiO2 particles can be evenly distributed on graphene slice layers, the graphene slice layers are not easy to overlap, dispersity is obviously improved, and meanwhile the performance that polyimide is good in heat resistance, high in mechanical performance, high in fire resistance and the like is achieved.

Description

technical field [0001] The invention relates to the field of composite materials, in particular to a graphene / SiO2 hybrid polyimide foam material and a preparation method thereof. Background technique [0002] Polyimide foam material is a kind of lightweight material with the best comprehensive performance of no smoke in fire, no flame spread, no toxicity and no release of poisonous gas. The polyimide material with a foam structure not only maintains the excellent heat resistance and flame retardancy of the original polyimide resin, but also has outstanding wave-transmitting properties, light weight, good flexibility and rebound, and convenient use. It can produce aircraft structural components, wings, bomb bay deceleration load-bearing plates, nozzle heat insulation sleeves, cabin flame-retardant insulation interlayers, pipe insulation layers, nuclear reactor radiation-proof partitions, etc., which are widely used in aviation, aerospace, and high-speed trains , automobiles...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C08L79/08C08K9/02C08K9/04C08K3/04C08K3/36C08G73/10C08J9/00
CPCC08G73/1071C08J9/00C08J2379/08C08K3/04C08K3/36C08K9/02C08K9/04C08L79/08
Inventor齐锴亮
Owner陕西工业职业技术学院